ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Ethylamine → 4,6-Dichloro-2-ethylamino-5-pyrimidinecarbonitrile

HRID 1757889
ノート
印刷プレビュー

反応式

HRID 1757889 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9]#[N:10])=[C:4]([Cl:11])[N:3]=1.[CH2:12]([NH2:14])[CH3:13]>CC(C)=O>[Cl:11][C:4]1[C:5]([C:9]#[N:10])=[C:6]([Cl:8])[N:7]=[C:2]([NH:14][CH2:12][CH3:13])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6341EthylamineHCID 2509452,4,6-Trichloro-5-cyanopyrimidine

生成物 1

HCID 205102564,6-Dichloro-2-ethylamino-5-pyrimidinecarbonitrile

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A stirred solution of 12.9 grams of 2,4,6-trichloro-5-pyrimidinecarbonitrile in 150 ml of acetone was cooled to -10°, and 7.7 grams of an aqueous 70% ethylamine solution was added dropwise during 2 hours. The temperature of the reaction mixture was maintained at -10° throughout the addition. Following complete addition, the reaction mixture was allowed to warm to room temperature, where it stood for 16 hours. Then most of the acetone was removed by evaporation under reduced pressure. The residue was extracted with a mixture of water and diethyl ether. The ether layer was separated and dried over magnesium sulfate. The dried ether layer was filtered, and the ether was removed under reduced pressure. The residue was recrystallized from a mixture of methylcyclohexane and benzene, then from carbon tetrachloride, to give 4.2 grams of 4,6-dichloro-2- ethylamino-5-pyrimidinecarbonitrile; mp, 145°-150°.

後処理

  1. temperatureThe temperature of the reaction mixture was maintained at -10° throughout the addition
  2. additionaddition
  3. customThen most of the acetone was removed by evaporation under reduced pressure
  4. extractionThe residue was extracted with a mixture of water and diethyl ether
  5. customThe ether layer was separated
  6. dry with materialdried over magnesium sulfate
  7. filtrationThe dried ether layer was filtered
  8. customthe ether was removed under reduced pressure
  9. customThe residue was recrystallized from a mixture of methylcyclohexane and benzene

出典と根拠

ORDレコード
ord-8dda806c88064b25898f344c54993db2
出典データセット
uspto-grants-1983_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE031136

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート